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Supercritical Fluid Treatment of High Molecular Weight Biopolymers

Active Publication Date: 2013-04-25
THE GOVERNORS OF THE UNIV OF ALBERTA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The invention describes a method for processing highly viscous aqueous solutions of HMW biopolymers into dry particles, agglomerates, and fibers using a pressurized chamber. The method involves spraying the solution together with a compressible gas and a water-soluble co-solvent / antisolvent into a chamber, where the solvent is removed through flushing with a second gas. The method can also be used to impregnate the particles with a bioactive material. The resulting micro- or nanoparticles have a high molecular weight and a low bulk density, making them useful in various applications such as food and medicine.

Problems solved by technology

However, such a low level of co-solvent is not sufficient to precipitate high molecular weight biopolymers such as polysaccharides.
Then, the expanded solution is rapidly depressurized to atmospheric conditions, resulting in the formation of sub-micron or micron sized solute crystals due to the very large temperature drop that occurs upon depressurization.
The prior art does not provide any solutions regarding the formation of micro / nano-sized particles, agglomerates or fibers (micro- or nanoparticles) from water-soluble high molecular weight (HMW) biopolymers, such as HMW gums and polysaccharides with molecular weights ranging from about 70,000 g / mol (70 kDa) up to over 1,000,000 g / mol (1,000 kDa), applying a SCF drying (SFD) and / or gas antisolvent (GAS) technique.
This is a major challenge, which complicates the spraying and atomization process involved in SFD and GAS.
Furthermore, the prior art is also silent when it comes to impregnation of such micro- or nanoparticles with bioactives or encapsulation of bioactives in micro- or nanoparticles made from such HMW biopolymers applying supercritical fluid technology for use in cosmetic, pharmaceutical, agricultural, nutraceutical or food products.

Method used

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  • Supercritical Fluid Treatment of High Molecular Weight Biopolymers
  • Supercritical Fluid Treatment of High Molecular Weight Biopolymers
  • Supercritical Fluid Treatment of High Molecular Weight Biopolymers

Examples

Experimental program
Comparison scheme
Effect test

example 1

Materials

[0071]Gum arabic (GA) was used as purchased without any further treatment (ACROS Organic, Fisher Scientific, Canada). β-Glucan (BG) powder (moisture content of 8.7% and BG content of 75% dry weight basis) previously extracted from barley in our lab according to the protocols described by Ghotra et al. [18] was used in the different experiments. Refined fish oil extracted from anchovy and sardine was obtained from Ocean Nutrition Canada (ONC, Halifax, NS, Canada) with a level of 8 and 25% for eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), respectively. Food grade anhydrous ethanol (Commercial Alcohol, Winnipeg, MB, Canada) with a stated purity and water content of 99.99% and 0.008% by volume, respectively, was used without further purification. Hexane of analytical grade (Fisher Scientific, Canada) was used for determining the lipid content of fish oil microcapsules. Bone dry CO2 with a purity of 99.9% and nitrogen with a purity of 99.998% were purchased from Pr...

example 2

Apparatus

[0072]The apparatus used for micro- or nanoparticle formation, microencapsulation and impregnation consisted of a 200 mL view cell with an internal diameter of 40 mm (Nova-Swiss, Effretikon, Switzerland) equipped with a coaxial-nozzle, temperature-controlled heaters and circulating air bath, shown schematically in FIG. 1. The system was pressurized with CO2 by means of a syringe pump (O) (Isco Model 260D, Isco Inc., Lincoln, Nebr.). CO2 was preheated to 45° C. using temperature-controlled electric heaters and mixed with ethanol, which was pumped into the system with an HPLC pump (T) (Gilson 305, HPLC pump, Gilson Inc., Middleton, Wis.).

[0073]The mixture of CO2+ethanol passed through a double-helix static mixer prior to injection into the view cell flowing in the outer channel of the coaxial nozzle (B). The flow rate of CO2 was adjusted using a heated metering valve (F) at the outlet of the view cell, and monitored by means of a rotameter (G), which was located after a seale...

example 3

Dry Particle Formation

[0079]Formation of micro- or nanoparticles, microencapsulation and impregnation experiments were carried out with the view cell preheated to 40° C., while the CO2+EtOH mixture was preheated to 45° C. in the tubing leading to the nozzle. The slightly higher temperature in the pre-heater was chosen to compensate for the cooling due to the Joule-Thomson effect during the expansion in the nozzle. The temperature in the spray chamber decreased during spraying from 40° C. to a constant value of about 38° C. For the particle formation experiments, various process parameters and conditions were evaluated during preliminary tests, including pressure, flow rates, nozzle setup, emulsifying device setup and concentration of solids in the aqueous solution as listed in Table 1. An overview of the experimental conditions studied is provided in Table 2.

[0080]In order to prepare dry nano-agglomerate particles from an aqueous solution containing 10% (w / w) GA, the GA solution was...

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Abstract

Micro- and nano-sized particles, agglomerates and fibers are generated from high molecular weight water-soluble biopolymers applying supercritical fluid technology. A method of producing micro- or nanoparticles from an aqueous solution of a high molecular weight biopolymer includes the step of spraying the aqueous solution together with a mixture of a compressible gas and a water-soluble co-solvent / antisolvent into a pressurized chamber. The method may be adapted to impregnate the micro- or nanoparticles with a bioactive material. A method for microencapsulating a bioactive material with a biopolymer is also provided.

Description

FIELD OF THE INVENTION[0001]The present invention is directed to methods of generating micro- and nano-sized particles, agglomerates and fibers from high molecular weight water-soluble biopolymers applying supercritical fluid technology. The invention further relates to the resulting products and methods of using the resulting products.BACKGROUND[0002]Particle formation using supercritical fluids has been researched for many decades, and has resulted in the development of numerous processes using the supercritical fluid (SCF) either as solvent, such as in the “rapid expansion of supercritical solutions” (RESS) process, as antisolvent in the “gas antisolvent” (GAS) process, or as co-solvent in the “depressurization of an expanded liquid organic solution” (DELOS) process. Numerous variations and further developments of particle formation processes have emerged [1-4]. However, many of these processes require organic solvents to dissolve the solute to be precipitated (US Patent Applicat...

Claims

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Application Information

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IPC IPC(8): C08J3/12B29B9/12
CPCA61K9/5089A61K9/5192C08J3/122Y10T428/2982C08J2305/00B29B9/12C08J3/12C08J3/215Y02P20/54
Inventor TEMELLI, FERALSEIFRIED, BERNHARD
Owner THE GOVERNORS OF THE UNIV OF ALBERTA
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